CN114835982A - High-gloss transparent sheet and preparation method thereof - Google Patents

High-gloss transparent sheet and preparation method thereof Download PDF

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Publication number
CN114835982A
CN114835982A CN202210549254.3A CN202210549254A CN114835982A CN 114835982 A CN114835982 A CN 114835982A CN 202210549254 A CN202210549254 A CN 202210549254A CN 114835982 A CN114835982 A CN 114835982A
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China
Prior art keywords
transparent sheet
parts
acr
sheet according
high gloss
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CN202210549254.3A
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Chinese (zh)
Inventor
何坤
孔阳
韦余康
董玉娇
倪青兰
陆伟
鲍晨
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Digaoli Decoration Materials Jiangsu Co ltd
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Digaoli Decoration Materials Jiangsu Co ltd
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Priority to CN202210549254.3A priority Critical patent/CN114835982A/en
Publication of CN114835982A publication Critical patent/CN114835982A/en
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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2327/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
    • C08J2327/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
    • C08J2327/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
    • C08J2327/06—Homopolymers or copolymers of vinyl chloride
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2423/04—Homopolymers or copolymers of ethene
    • C08J2423/06—Polyethene
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2423/26—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers modified by chemical after-treatment
    • C08J2423/28—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers modified by chemical after-treatment by reaction with halogens or halogen-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
    • C08J2433/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/09—Carboxylic acids; Metal salts thereof; Anhydrides thereof
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/10—Esters; Ether-esters
    • C08K5/11—Esters; Ether-esters of acyclic polycarboxylic acids
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K5/00—Use of organic ingredients
    • C08K5/04—Oxygen-containing compounds
    • C08K5/10—Esters; Ether-esters
    • C08K5/12—Esters; Ether-esters of cyclic polycarboxylic acids

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Casting Or Compression Moulding Of Plastics Or The Like (AREA)

Abstract

The invention discloses a high-gloss transparent sheet and a preparation method thereof, which can reduce the dosage of a plasticizer and effectively increase the surface hardness of the transparent sheet so as to reduce the microscopic roughness of the surface of the substrate in the hot pressing process. The ACR auxiliary agent is added into the preparation raw materials, so that the gloss effect of the surface of the transparent sheet is effectively improved, and the toughness of the transparent sheet is increased to a certain extent. Due to the increased hardness, the CPE synergistically improved the toughness of the transparency with the ACR. The ACR part of the processing aid is greatly improved, the stability of PVC in the plasticizing process needs to be improved, the anti-aging performance is improved, and further, the frictional heat in the plasticizing process is reduced by adding stearic acid and PE wax serving as internal and external synergistic lubricants.

Description

High-gloss transparent sheet and preparation method thereof
Technical Field
The invention relates to the field of preparation of transparent sheets of floor accessories, in particular to a high-gloss transparent sheet and a preparation method thereof.
Background
The hard PVC floor is made up by using natural stone powder and resin powder as base material, covering the surface with high-molecular wear-resisting layer and adopting several procedures of high-temp. hot-pressing and hot-pressing, etc. and has no need of using substances containing formaldehyde and toluene, such as glue and paint. The hard PVC floor is popular in developed countries in Europe and America and the Asia-Tai market, is derived from German brand 'JOKA Jinjia' SPC silent floor by virtue of excellent stability and durability, not only solves the problems of damp deformation and mildew of solid wood floors, but also solves the environmental protection problems of formaldehyde and the like of other decoration materials, meets the use requirements of high-end customers in China, and is a representative of a novel high-tech floor material in the twenty-first century. It is obvious from the trend of products developed by floor enterprises in China and abroad in recent two years that more and more floor enterprises are transformed or extended to the production and sale of hard PVC floors, the product lines of various large brands are adjusted, and the hard PVC floors gradually replace the existing common ground materials and become a new favorite in the tooling and home decoration markets.
If the marble-imitated plastic floor is to be produced, the key technical point lies in the development of the high-gloss wear-resistant layer transparent sheet, and the transparent sheets on the market at present are all high-haze low-hardness PVC transparent sheets. But not for the preparation of high-gloss plastic floors.
Disclosure of Invention
The purpose of the invention is as follows: in order to solve the problems in the prior art, the invention provides a high-gloss transparent sheet with high gloss, high transparency and high hardness and a preparation method thereof.
The technical scheme is as follows: in order to achieve the above purpose, the invention adopts the following technical scheme: the highlight transparent sheet has the advantages that the usage amount of a plasticizer is reduced in preparation raw materials, and the specific reduction ratio is 25-50%; the ACR auxiliary agent is also added into the preparation raw materials.
Furthermore, the preparation raw materials specifically comprise the following components in parts by weight: 80-100 parts of PVC resin, 10-15 parts of plasticizer, 3-7 parts of ACR (acrylate copolymer) additive, 3-5 parts of CPE (chlorinated polyethylene), 1.5-3 parts of stabilizer, 0.1-0.3 part of PE (polyethylene) wax, 0.2-0.5 part of stearic acid and 0.2-0.9 part of anti-ultraviolet agent.
Further, the PVC resin is low-polymerization-degree resin powder with a K value of 57 or 60.
Further, the plasticizer is at least one of dioctyl adipate, diisooctyl adipate, dioctyl terephthalate, dioctyl phthalate and dioctyl phthalate.
Further, the ACR auxiliary agent adopts low molecular weight ACR 401.
The invention also discloses a preparation method of the highlight transparent sheet, which comprises the following steps:
(1) dry mixing: feeding all materials according to a formula, and uniformly mixing in a high-speed mixer at the mixing temperature of 100-125 ℃;
(2) extruding and plasticizing: putting the uniformly mixed material into an extruder with a T-shaped neck mold for plasticizing;
(3) thickness setting: the flaky fluid coming out from the T-shaped neck mold is subjected to calender thickness setting; wherein the surface smoothness of a roller of the calender reaches 12;
(4) cooling and rolling: and cooling the highlight transparent sheet by a cooling roller to obtain a finished highlight transparent sheet product.
Furthermore, the temperature of the extruder in the step (2) is adjusted to 155-175 ℃.
Furthermore, the working parameters of the calender in the step (3) are that the calendering temperature is 170-190 ℃, the calendering speed of a roller is 5-15 m/min, and the calendering speed ratio is 1.01-1.20.
Has the advantages that:
(1) the invention reduces the dosage of the plasticizer, effectively increases the surface hardness of the transparent sheet, and reduces the microscopic roughness of the surface of the substrate in the hot pressing process.
(2) The ACR auxiliary agent is added into the preparation raw materials, so that the gloss effect of the surface of the transparent sheet is effectively improved, and the toughness of the transparent sheet is increased to a certain extent.
(3) The CPE synergistically improved the toughness of the transparency with the ACR due to the increased hardness. The ACR part of the processing aid is greatly improved, the stability of PVC in the plasticizing process needs to be improved, the anti-aging performance is improved, and further, the frictional heat in the plasticizing process is reduced by adding stearic acid and PE wax serving as internal and external synergistic lubricants.
Detailed Description
Example 1:
a preparation method of a high-gloss transparent sheet comprises the following steps:
(1) dry mixing: feeding all materials according to a formula, and uniformly mixing in a high-speed mixer at the mixing temperature of 100 ℃; the preparation raw materials comprise the following components in parts by weight: 80 parts of PVC resin, 10 parts of plasticizer, 3 parts of ACR (acrylic resin) additive, 3 parts of CPE (chlorinated polyethylene), 1.5 parts of stabilizer, 0.1 part of PE (polyethylene) wax, 0.2 part of stearic acid and 0.2 part of ultraviolet inhibitor; the PVC resin is low-polymerization-degree resin powder with a K value of 57 or 60; the plasticizer is dioctyl adipate; the ACR auxiliary agent adopts ACR401 with low molecular weight;
(2) extruding and plasticizing: putting the uniformly mixed material into an extruder with a T-shaped neck mold for plasticizing; the extruder adjusted the press temperature to 155 ℃.
(3) Thickness setting: the flaky fluid coming out from the T-shaped neck mold is subjected to calender thickness setting; wherein the surface smoothness of a roller of the calender reaches 12; the working parameters of the calender are that the calendering temperature is 170 ℃, the calendering speed of one roller is 5m/min, and the calendering speed ratio is 1.01;
(4) cooling and rolling: and cooling the highlight transparent sheet by a cooling roller to obtain a finished highlight transparent sheet product.
Example 2:
a preparation method of a high-gloss transparent sheet comprises the following steps:
(1) dry mixing: feeding all materials according to a formula, and uniformly mixing in a high-speed mixer at a mixing temperature of 125 ℃; the preparation raw materials comprise the following components in parts by weight: 100 parts of PVC resin, 15 parts of plasticizer, 7 parts of ACR (acrylic resin) additive, 5 parts of CPE (chlorinated polyethylene), 3 parts of stabilizer, 0.3 part of PE (polyethylene) wax, 0.5 part of stearic acid and 0.9 part of ultraviolet inhibitor; the PVC resin is low-polymerization-degree resin powder with a K value of 57 or 60; the plasticizer is dioctyl phthalate; the ACR auxiliary agent adopts ACR401 with low molecular weight;
(2) extruding and plasticizing: putting the uniformly mixed material into an extruder with a T-shaped neck mold for plasticizing; the extruder adjusted the press temperature to 175 ℃.
(3) Thickness setting: the flaky fluid coming out from the T-shaped neck mold is subjected to calender thickness setting; wherein the surface smoothness of a roller of the calender reaches 12; the working parameters of the calender are that the calendering temperature is 190 ℃, the calendering one-roll speed is 15m/min, and the calendering speed ratio is 1.20;
(4) cooling and rolling: and cooling the highlight transparent sheet by a cooling roller to obtain a finished highlight transparent sheet product.
Example 3:
a preparation method of a high-gloss transparent sheet comprises the following steps:
(1) dry mixing: feeding all materials according to a formula, and uniformly mixing in a high-speed mixer at the mixing temperature of 115 ℃; the preparation raw materials comprise the following components in percentage by weight: 90 parts of PVC resin, 12 parts of plasticizer, 5 parts of ACR (acrylic resin) additive, 4 parts of CPE (chlorinated polyethylene), 2 parts of stabilizer, 0.2 part of PE (polyethylene) wax, 0.4 part of stearic acid and 0.5 part of ultraviolet inhibitor; the PVC resin is low-polymerization-degree resin powder with a K value of 57 or 60; the plasticizer is diisooctyl adipate; the ACR auxiliary agent adopts ACR401 with low molecular weight;
(2) extruding and plasticizing: putting the uniformly mixed material into an extruder with a T-shaped neck mold for plasticizing; the extruder adjusts the press temperature to 160 ℃.
(3) Thickness setting: the flaky fluid coming out from the T-shaped neck mold is subjected to calender thickness setting; wherein the surface smoothness of a roller of the calender reaches 12; the working parameters of the calender are that the calendering temperature is 180 ℃, the calendering one-roll speed is 10m/min, and the calendering speed ratio is 1.1;
(4) cooling and rolling: and cooling the highlight transparent sheet by a cooling roller to obtain a finished highlight transparent sheet product.
With the addition of comparative examples 1 and 2,
comparative example 1:
other embodiments are the same as example 3, except that the plasticizer is used in an amount of 25 parts.
Comparative example 2:
other embodiments are the same as example 3, except that no ACR401 adjuvant is added.
The performance of the floor finished products prepared in the example 3 and the comparative examples 1-2 is tested, the specific performance indexes are glossiness, hardness, elongation at break, dimensional stability and the like, and the glossiness instrument, the hardness instrument, the stretcher, the forced air oven and the like are respectively used for testing;
the test results are shown in table 1:
table 1, comprehensive performance test results of floor finished products in example 3 and comparative examples 1-2
Test index Example 3 Comparative example 1 Comparative example 2
Degree of gloss 82 30 20
Hardness of 92 82 19
Elongation at break% 156 260 315
Shrinkage in size% 0.4 1.2 1.5
As can be seen from the data in table 1, compared with comparative examples 1-2, the amount of the plasticizer used in the preparation process of the highlight transparent sheet prepared in example 3 of the present invention is reduced, so that the surface hardness of the transparent sheet is effectively increased, the microscopic roughness of the surface of the floor in the hot pressing process is reduced, the glossiness of the floor is significantly improved, and the good scratch and dent resistance of the surface of the floor in the using process is ensured.

Claims (8)

1. A highlight transparent sheet is characterized in that the use amount of a plasticizer is reduced in preparation raw materials, and the specific reduction ratio is 25-50%; the ACR auxiliary agent is also added into the preparation raw materials.
2. The highlight transparent sheet according to claim 1, characterized by comprising the following preparation raw materials by weight: 80-100 parts of PVC resin, 10-15 parts of plasticizer, 3-7 parts of ACR (acrylate copolymer) additive, 3-5 parts of CPE (chlorinated polyethylene), 1.5-3 parts of stabilizer, 0.1-0.3 part of PE (polyethylene) wax, 0.2-0.5 part of stearic acid and 0.2-0.9 part of anti-ultraviolet agent.
3. The high gloss transparent sheet according to claim 2, wherein: the PVC resin is low-polymerization-degree resin powder with a K value of 57 or 60.
4. The high gloss transparent sheet according to claim 1 or 2, wherein: the plasticizer is at least one of dioctyl adipate, diisooctyl adipate, dioctyl terephthalate, dioctyl phthalate and dioctyl phthalate.
5. The high gloss transparent sheet according to claim 1 or 2, wherein: the ACR auxiliary agent adopts ACR401 with low molecular weight.
6. A method for preparing a high gloss transparent sheet according to claim 1, comprising the steps of:
(1) dry mixing: feeding all materials according to a formula, and uniformly mixing in a high-speed mixer at the mixing temperature of 100-;
(2) extruding and plasticizing: putting the uniformly mixed material into an extruder with a T-shaped neck mold for plasticizing;
(3) thickness setting: the flaky fluid coming out from the T-shaped neck mold is subjected to calender thickness setting; wherein the surface smoothness of a roller of the calender reaches 12;
(4) cooling and rolling: and cooling the highlight transparent sheet by a cooling roller to obtain a finished highlight transparent sheet product.
7. The method for producing a high gloss transparent sheet according to claim 6, wherein: in the step (2), the temperature of the extruder is adjusted to be 155-175 ℃.
8. The method for producing a high gloss transparent sheet according to claim 6, wherein: the working parameters of the calender in the step (3) are that the calendering temperature is 170-190 ℃, the speed of a calendering roller is 5-15 m/min, and the calendering speed ratio is 1.01-1.20.
CN202210549254.3A 2022-05-20 2022-05-20 High-gloss transparent sheet and preparation method thereof Pending CN114835982A (en)

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Application Number Priority Date Filing Date Title
CN202210549254.3A CN114835982A (en) 2022-05-20 2022-05-20 High-gloss transparent sheet and preparation method thereof

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103289230A (en) * 2013-05-29 2013-09-11 新疆天业（集团）有限公司 Transparent polyvinyl chloride (PVC) granule and production method thereof
WO2017121389A1 (en) * 2016-01-15 2017-07-20 上海协承昌化工有限公司 Composite floor
CN112895642A (en) * 2021-01-26 2021-06-04 浙江海利得地板有限公司 Micro-foaming PVC floor without plasticizer and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103289230A (en) * 2013-05-29 2013-09-11 新疆天业（集团）有限公司 Transparent polyvinyl chloride (PVC) granule and production method thereof
WO2017121389A1 (en) * 2016-01-15 2017-07-20 上海协承昌化工有限公司 Composite floor
CN112895642A (en) * 2021-01-26 2021-06-04 浙江海利得地板有限公司 Micro-foaming PVC floor without plasticizer and preparation method thereof

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Application publication date: 20220802